CN101089249A - Preparation and application of cellulose mixed fibre using ion liquid as solvent - Google Patents
Preparation and application of cellulose mixed fibre using ion liquid as solvent Download PDFInfo
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- CN101089249A CN101089249A CN 200710043563 CN200710043563A CN101089249A CN 101089249 A CN101089249 A CN 101089249A CN 200710043563 CN200710043563 CN 200710043563 CN 200710043563 A CN200710043563 A CN 200710043563A CN 101089249 A CN101089249 A CN 101089249A
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Abstract
The present invention relates to a method for preparing cellulose polyblend fiber by using ionic liquid as solvent and its application method. Said preparation method includes the following steps: (1), uniformly mixing pulverized cellulose, chitin/chitosan and ionic liquid, dissolving them for 1-80 h at 25-160 deg.C so as to obtain the uniform stable spinning solution whose total solid content is 3-40%; (2), filtering and defoaming, then making the spinning solution be passed through single-hole or multi-hole spinneret, and fed into a coagulating bath and solidified, its spinning speed is 5-150 m/min; and (3), plasticizing, drawing, washing, bleaching, oiling and drying so as to obtain the invented cellulose polyblend fiber product. The spinning solution prepared by aid invention also can be used for preparing hollow fiber membrane, specially, can be used for making artificial organ and membrane for water purifier.
Description
Technical field
The invention belongs to the preparation and the application of cellulose blending fibre, particularly relating to a kind of is the preparation and the application of the cellulose blending fibre of solvent with the ionic liquid.
Background technology
Not only storage level is big for cellulose in all substances of occurring in nature, and huge amount of recovery is arranged.Have only few cellulose to be made into fiber at present, be used to make the cellulose amount of fiber and film, 4% of the cellulose output of producing no more than world industry.Along with the mankind to the deepening continuously and the worsening shortages of resources such as oil, coal, natural gas of nature understanding, cellulosic utilization also will enlarge gradually.
Cellulose fibre is because raw cellulose can be changed into steam and carbon dioxide by biological decomposition or safe combustion, and the destruction environmental problem that is caused by discarded object is few, and it is very necessary therefore developing cellulose fibre.What at present produce cellulose fibers mainly adopted is viscose process, and production process is tediously long and complicated, energy consumption and operating cost height, and exist waste gas, waste water, waste residue pollution, handle multinomial problem such as recovery.
Ionic liquid exists with liquid state in the scope of broad as a kind of novel cellulose solvent, and has good heat endurance, and nontoxic, non-volatility helps environmental protection and operator ' s health.Yin, yang ion population by selecting to suit can change ion liquid physicochemical properties, thereby dissolves multiple organic matter, inorganic matter and macromolecular material.Many ionic liquids are very big to cellulosic solubility, some in addition reach 35%, but adopt cellulose yellow method to produce the cellulose concentration that viscose adopted and be no more than 10%, therefore, adopt the ionic liquid produce cellulose fibers to enhance productivity greatly.
The cellulose blending fibre that sees report at present reports that seldom majority utilizes cellulose fibre and other fiber blends to produce.
Functions such as that chitin, shitosan have is antibacterial, antipruritic, deodorization, smelly, the anti-inflammatory of disappearing, pain relieving, but one piece of report that adopts viscose process to prepare the cellulose/chitin blending fiber is only arranged.
Summary of the invention
The purpose of this invention is to provide a kind of is the methods and applications that cosolvent prepares cellulose blending fibre with the ionic liquid, and this method is low in the pollution of the environment, can satisfy the production needs.
Of the present invention a kind of be the cellulose blending fibre preparation method of solvent with the ionic liquid, comprise the following steps:
(1) comminuted fibres element, chitin/chitosan and ionic liquid mix, and dissolve 1～80 hour under 25～160 ℃ of temperature, and the formation total solid content is 3～40% stable homogeneous spinning solution;
(2) filter, after the deaeration, enter in the coagulating bath through the porous spinnerets and to solidify, spinning speed be 5～150m rice/minute;
(3) behind plasticization drawing, again through wash, bleach, oil, drying, the cellulose blending fibre goods.
Described cellulose is selected from a kind of in bamboo pulp, wood pulps, the cotton pulp dregs of rice, reed pulp, bagasse pulp or the jute bar slurry, and the degree of polymerization is 300～2500, alpha-cellulose content 〉=90%;
Described chitin/chitosan η=20～35cps, granularity≤4mm, purity 〉=90%, protein≤0.5%, ash≤1%, with cellulosic mixed proportion be 99: 1～1: 99;
Described ionic liquid is made up of CATION and anion;
Described CATION is that substituting group is hydrogen, C
1～C
6Alkyl, vinyl, propenyl, cyclobutenyl, ethoxy, hydroxypropyl, alkoxyl in one or more quaternary ammonium alkyl ion, alkyl quaternary phosphonium ion, alkyl imidazole ion, alkyl pyridine ion;
Described anion is halide ion, BF
4 -, PF
4 -, SCN
-, CN
-, OCN
-, CNO
-, CF
3SO
3 -, CF
3COO
-, (CF
3SO
2)
2N
-Or (CF
3SO
2)
2Cl
-In a kind of;
Described coagulating bath is the ionic liquid aqueous solution of water or 0～60%, and coagulation bath temperature is 0～90 ℃;
Described stretching is selected from one or more in nervous stretching, jet stretch, plasticization drawing, air bath after-drawing or the retraction, and total drawing ratio is 10-200%.
Of the present invention is the preparation that the cellulose blending spinning solution of solvent also can be used for doughnut with the ionic liquid, especially for the film of using of manufacture of intraocular internal organs and water purifier.
Beneficial effect of the present invention:
(1) adopt ionic liquid to prepare fiber, avoided the tediously long and complicated production process of viscose process, production process obviously shortens, and process energy consumption and operating cost are low, and help environmental protection and operator ' s health, meet the requirement of green production;
(2) the preparation-obtained cellulose blending fibre of the present invention has excellent mechanical intensity, the conventional viscose that its mechanical performance is produced apparently higher than corresponding employing viscose process;
(3) blended fiber also can be made underwear, handkerchief, can be made into various garment materials through blending or pure spinning.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
9.95 parts of pulps pulverizing, 0.05 part of chitin are mixed, mix, stirred 24 hours down, obtain spinning solution at 45 ℃ with 100 parts of [BMIM] Cl ionic liquids.Spinning solution after filtration, after the deaeration, enter into through the porous spinnerets and to contain 5% ion liquid coagulating bath, coagulation bath temperature is 25 ℃.Behind 10% plasticization drawing, again through wash, bleach, oil, dry supervisor, spinning speed is 5 meters/minute, obtains the fiber that intensity is 3.2cN/dtex.
Embodiment 2
9 parts of pulps pulverizing, 1 part of chitin are mixed, mix, stirred 120 hours down, obtain spinning solution at 100 ℃ with 200 parts of [BMIM] Cl ionic liquids.Spinning solution after filtration, after the deaeration, enter into the water coagulating bath through the porous spinnerets, coagulation bath temperature is 15 ℃.Behind 1% plasticization drawing, again through wash, bleach, oil, dry supervisor, spinning speed is 20 meters/minute, obtains the fiber that intensity is 3.5cN/dtex.
Embodiment 3
9 parts of pulps pulverizing, 1 part of chitin are mixed, mix, stirred 80 hours down, obtain spinning solution at 60 ℃ with 40 parts of [AMIM] Br ionic liquids.Spinning solution after filtration, after the deaeration, enter into through the porous spinnerets and to contain 25% ion liquid coagulating bath, coagulation bath temperature is 55 ℃.Behind 8% plasticization drawing, again through wash, bleach, oil, dry supervisor, spinning speed is 30 meters/minute, obtains the fiber that intensity is 4.0cN/dtex.
Embodiment 4
9 parts of pulps pulverizing, 1 part of chitin are mixed, mix, stirred 50 hours down, obtain spinning solution at 150 ℃ with 90 parts of [AMIM] Cl ionic liquids.Spinning solution after filtration, after the deaeration, enter into through the porous spinnerets and to contain 45% ion liquid coagulating bath, coagulation bath temperature is 85 ℃.Behind 5% plasticization drawing, again through wash, bleach, oil, dry supervisor, spinning speed is 40 meters/minute, obtains the fiber that intensity is 2.3cN/dtex.
Claims (8)
1. one kind is the cellulose blending fibre preparation method of solvent with the ionic liquid, comprises the following steps:
(1) comminuted fibres element, chitin/chitosan and ionic liquid mix, and dissolve 1～80 hour under 25～160 ℃ of temperature, and the formation total solid content is 3～40% stable homogeneous spinning solution;
(2) filter, after the deaeration, enter in the coagulating bath through single hole or porous spinnerets and to solidify, spinning speed be 5～150m rice/minute;
(3) behind plasticization drawing, again through wash, bleach, oil, drying, obtain the cellulose blending fibre goods.
2. according to claim 1 a kind of be the cellulose blending fibre preparation method of solvent with the ionic liquid, it is characterized in that: described cellulose is selected from a kind of in bamboo pulp, wood pulps, the cotton pulp dregs of rice, reed pulp, bagasse pulp or the jute bar slurry, the degree of polymerization is 300～2500, alpha-cellulose content 〉=90%.
3. according to claim 1 a kind of be the cellulose blending fibre preparation method of solvent with the ionic liquid, it is characterized in that: described chitin/chitosan η=20～35cps, granularity≤4mm, purity 〉=90%, protein≤0.5%, ash≤1%, with cellulosic mixed proportion be 99: 1～1: 99.
4. according to claim 1 a kind of be the cellulose blending fibre preparation method of solvent with the ionic liquid, it is characterized in that: described ionic liquid is made up of CATION and anion, CATION is that substituting group is hydrogen, C
1～C
6Alkyl, vinyl, propenyl, cyclobutenyl, ethoxy, hydroxypropyl, alkoxyl in one or more quaternary ammonium alkyl ion, alkyl quaternary phosphonium ion, alkyl imidazole ion, alkyl pyridine ion; Anion is halide ion, BF
4 -, PF
4 -, SCN
-, CN
-, OCN
-, CNO
-, CF
3SO
3 -, CF
3COO
-, (CF
3SO
2)
2N
-Or (CF
3SO
2)
2Cl
-In a kind of.
5. according to claim 1 a kind of be the cellulose blending fibre preparation method of solvent with the ionic liquid, it is characterized in that: described coagulating bath is the ionic liquid aqueous solution of water or 0～60%, coagulation bath temperature is 0～90 ℃.
6. according to claim 1 a kind of be the cellulose blending fibre preparation method of solvent with the ionic liquid, it is characterized in that: described stretching is selected from one or more in nervous stretching, jet stretch, plasticization drawing, air bath after-drawing or the retraction, and total drawing ratio is 10-200%.
7. according to claim 1 a kind of be the method that solvent prepares bamboo pulp fiber with the ionic liquid, it is characterized in that: the spinning process that is adopted is wet spinning, melt and spray wet spinning or dry-jet wet spinning.
8. one kind is the bamboo pulp fiber of solvent preparation with the ionic liquid, is used for the film of using of manufacture of intraocular internal organs and water purifier.
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|---|---|---|---|
| CN 200710043563 CN101089249A (en) | 2007-07-06 | 2007-07-06 | Preparation and application of cellulose mixed fibre using ion liquid as solvent |
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|---|---|---|---|
| CN 200710043563 CN101089249A (en) | 2007-07-06 | 2007-07-06 | Preparation and application of cellulose mixed fibre using ion liquid as solvent |
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Cited By (20)
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|---|---|---|---|---|
| EP2199319A1 (en) | 2008-12-19 | 2010-06-23 | Gambro Lundia AB | Virus filter |
| CN101899171A (en) * | 2010-08-20 | 2010-12-01 | 厦门大学 | Method for preparing chitosan/cellulose composite material |
| CN101274268B (en) * | 2007-12-29 | 2011-03-30 | 中国科学院长春应用化学研究所 | Producing method of biological adsorbing agent with adsorption capacity of heavy metal ion |
| CN102168323A (en) * | 2011-02-24 | 2011-08-31 | 天津工业大学 | Method for preparing chitosan and chitin functional materials by taking ionic liquid as solvent |
| CN101748499B (en) * | 2008-12-05 | 2011-10-05 | 中国纺织科学研究院 | Chitin fiber and preparation method thereof |
| CN101748503B (en) * | 2008-12-18 | 2011-11-16 | 中国纺织科学研究院 | Method for preparing chitin/acrylic composite fiber by using ionic liquid as solvent |
| CN102251302A (en) * | 2011-05-28 | 2011-11-23 | 东华大学 | Preparation method of cellulose diacetate fiber |
| CN101768790B (en) * | 2008-12-29 | 2011-12-28 | 中国纺织科学研究院 | Sheath core composite fibre of chitin and cellulose and preparation method thereof |
| CN102532346A (en) * | 2011-12-30 | 2012-07-04 | 沈阳药科大学 | Environmentally-friendly method for preparing chitosan quaternary ammonium salt in ion liquid |
| CN102560741A (en) * | 2012-01-12 | 2012-07-11 | 大连工业大学 | Chitosan and polyvinyl pyrrolidone (PVP) blended fiber and preparation method thereof |
| CN102619026A (en) * | 2012-04-20 | 2012-08-01 | 天津工业大学 | Preparation method of nano micro cellulose fiber non-woven fabric |
| CN102704038A (en) * | 2012-06-21 | 2012-10-03 | 大连工业大学 | Cyanoethyl chitosan fiber and preparation method thereof |
| CN102828283A (en) * | 2012-09-10 | 2012-12-19 | 东华大学 | Method for preparing chitosan and cellulose complex fibers by binary solvent system |
| CN102936762A (en) * | 2012-10-22 | 2013-02-20 | 中国纺织科学研究院 | Preparation method of chitosan/cellulose homogeneous spinning solution |
| CN103183832A (en) * | 2011-12-28 | 2013-07-03 | 中国科学院青岛生物能源与过程研究所 | Preparation method for magnetic cellulose-chitosan composite microsphere |
| CN104451941A (en) * | 2014-12-01 | 2015-03-25 | 恒天海龙股份有限公司 | Carboxymethyl chitosan/cellulose composite material and preparation method thereof |
| CN104762680A (en) * | 2015-03-26 | 2015-07-08 | 苏州威尔德工贸有限公司 | Regenerated protein fiber containing ionic liquid |
| CN105839273A (en) * | 2016-04-29 | 2016-08-10 | 华南再生棉纱（梧州）有限公司 | Bamboo fiber flax towel manufacturing method |
| CN110359111A (en) * | 2019-07-19 | 2019-10-22 | 嘉兴学院 | Chitosan and/or its derivative modified regenerated celulose fibre and preparation method thereof |
| CN113652759A (en) * | 2021-05-06 | 2021-11-16 | 北京林业大学 | Regenerated antibacterial fiber non-woven fabric and preparation method and application thereof |
-
2007
- 2007-07-06 CN CN 200710043563 patent/CN101089249A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101274268B (en) * | 2007-12-29 | 2011-03-30 | 中国科学院长春应用化学研究所 | Producing method of biological adsorbing agent with adsorption capacity of heavy metal ion |
| CN101748499B (en) * | 2008-12-05 | 2011-10-05 | 中国纺织科学研究院 | Chitin fiber and preparation method thereof |
| CN101748503B (en) * | 2008-12-18 | 2011-11-16 | 中国纺织科学研究院 | Method for preparing chitin/acrylic composite fiber by using ionic liquid as solvent |
| EP2199319A1 (en) | 2008-12-19 | 2010-06-23 | Gambro Lundia AB | Virus filter |
| CN101768790B (en) * | 2008-12-29 | 2011-12-28 | 中国纺织科学研究院 | Sheath core composite fibre of chitin and cellulose and preparation method thereof |
| CN101899171A (en) * | 2010-08-20 | 2010-12-01 | 厦门大学 | Method for preparing chitosan/cellulose composite material |
| CN102168323A (en) * | 2011-02-24 | 2011-08-31 | 天津工业大学 | Method for preparing chitosan and chitin functional materials by taking ionic liquid as solvent |
| CN102251302A (en) * | 2011-05-28 | 2011-11-23 | 东华大学 | Preparation method of cellulose diacetate fiber |
| CN103183832B (en) * | 2011-12-28 | 2015-11-18 | 中国科学院青岛生物能源与过程研究所 | A kind of preparation method of magnetic cellulose-chitosan composite microsphere |
| CN103183832A (en) * | 2011-12-28 | 2013-07-03 | 中国科学院青岛生物能源与过程研究所 | Preparation method for magnetic cellulose-chitosan composite microsphere |
| CN102532346A (en) * | 2011-12-30 | 2012-07-04 | 沈阳药科大学 | Environmentally-friendly method for preparing chitosan quaternary ammonium salt in ion liquid |
| CN102560741A (en) * | 2012-01-12 | 2012-07-11 | 大连工业大学 | Chitosan and polyvinyl pyrrolidone (PVP) blended fiber and preparation method thereof |
| CN102560741B (en) * | 2012-01-12 | 2014-04-09 | 大连工业大学 | Chitosan and polyvinyl pyrrolidone (PVP) blended fiber and preparation method thereof |
| CN102619026A (en) * | 2012-04-20 | 2012-08-01 | 天津工业大学 | Preparation method of nano micro cellulose fiber non-woven fabric |
| CN102704038A (en) * | 2012-06-21 | 2012-10-03 | 大连工业大学 | Cyanoethyl chitosan fiber and preparation method thereof |
| CN102828283A (en) * | 2012-09-10 | 2012-12-19 | 东华大学 | Method for preparing chitosan and cellulose complex fibers by binary solvent system |
| CN102936762B (en) * | 2012-10-22 | 2015-04-08 | 中国纺织科学研究院 | Preparation method of chitosan/cellulose homogeneous spinning solution |
| CN102936762A (en) * | 2012-10-22 | 2013-02-20 | 中国纺织科学研究院 | Preparation method of chitosan/cellulose homogeneous spinning solution |
| CN104451941A (en) * | 2014-12-01 | 2015-03-25 | 恒天海龙股份有限公司 | Carboxymethyl chitosan/cellulose composite material and preparation method thereof |
| CN104451941B (en) * | 2014-12-01 | 2017-03-15 | 恒天海龙（潍坊）新材料有限责任公司 | Carboxymethyl chitosan/cellulose composite material and preparation method thereof |
| CN104762680A (en) * | 2015-03-26 | 2015-07-08 | 苏州威尔德工贸有限公司 | Regenerated protein fiber containing ionic liquid |
| CN105839273A (en) * | 2016-04-29 | 2016-08-10 | 华南再生棉纱（梧州）有限公司 | Bamboo fiber flax towel manufacturing method |
| CN110359111A (en) * | 2019-07-19 | 2019-10-22 | 嘉兴学院 | Chitosan and/or its derivative modified regenerated celulose fibre and preparation method thereof |
| CN110359111B (en) * | 2019-07-19 | 2021-11-19 | 嘉兴学院 | Chitosan and/or derivative thereof modified regenerated cellulose fiber and preparation method thereof |
| CN113652759A (en) * | 2021-05-06 | 2021-11-16 | 北京林业大学 | Regenerated antibacterial fiber non-woven fabric and preparation method and application thereof |
| CN113652759B (en) * | 2021-05-06 | 2023-04-07 | 北京林业大学 | Regenerated antibacterial fiber non-woven fabric and preparation method and application thereof |
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